As an emerging electrode, metal-organic frameworks (MOFs) with the advantages of adjustable structures and high porosity have promising application in supercapacitors (SCS). Two novel MOFs, namely, {[Co-2(TCPB)(bisp)(mu(3)-OH)]center dot H2O center dot 2Dioxane}(n) (1) and {[Co-1.5(TCPB)(bisp)(1.5)(H2O)]center dot DMF}(n) (2) {H3TCPB = 1,3,5-tris(4-carbonylphenyloxy)benzene, bisp = 1.4-bis(pyrid-4-yl)benzene)}, have been synthesized under solvothermal conditions by regulating reaction temperature. X-ray diffraction analysis shows that MOF 1 is a twofold interpenetrated 3D architecture with the point symbol of {4(3)}(2){4(6).6(18).8(4)}, while MOF 2 is a novel 3-nodal (3,4,6)-c {4.8(2)}(2){4(2).6(8).8(3).10(2)}{8 X 10(5)} net. Meanwhile, the electrochemical properties of MOFs and MOFs@GO electrodes were measured. The results show that the electrochemical performance of 1 is better than that of 2, which may due to the structural differences caused by different reaction temperatures, and MOFs@GO-based electrodes present higher pseudocapacitance than those of MOFs-based electrodes, which is attributed to the complementary and synergistic effects of the advantages of both GO and MOFs. Furthermore, the relationship between the doping amount of GO and the specific capacitance of MOFs@GO-x%-based electrodes indicates that the specific capacitance of the electrode is not proportional to the doping amount of GO. The specific capacitance is the largest when the doping amount of GO is 5%. This work provides a new strategy for the potential application of MOFs-based electrodes for SCS by adjusting synthesis temperature of MOFs.